CN111916734B - Chromium-based sulfoselenide positive electrode material and preparation method and application thereof - Google Patents

Chromium-based sulfoselenide positive electrode material and preparation method and application thereof Download PDF

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CN111916734B
CN111916734B CN202010658779.1A CN202010658779A CN111916734B CN 111916734 B CN111916734 B CN 111916734B CN 202010658779 A CN202010658779 A CN 202010658779A CN 111916734 B CN111916734 B CN 111916734B
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chromium
positive electrode
sulfoselenide
ion battery
electrode material
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CN111916734A (en
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杨思宇
史鼎任
傅正文
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Fuyang Solid State Energy Storage Technology Liyang Co ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/581—Chalcogenides or intercalation compounds thereof
    • H01M4/5815—Sulfides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00—Selenium; Tellurium; Compounds thereof
    • C01B19/002—Compounds containing, besides selenium or tellurium, more than one other element, with -O- and -OH not being considered as anions
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/581—Chalcogenides or intercalation compounds thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention relates to a chromium-based sulfoselenide positive electrode material and a preparation method and application thereofxSe2‑xWherein x is more than 0 and less than 2; the chromium-based sulfoselenide positive electrode material is used as a positive electrode material of a metal ion battery, and the metal ion battery comprises any one of a sodium ion battery, a lithium ion battery, a potassium ion battery, a magnesium ion battery, an aluminum ion battery and a calcium ion battery. The chromium-based sulfoselenide positive electrode material provided by the invention has a layered structure, not only has higher specific capacity, but also has excellent rate capability, and meanwhile, the chromium-based sulfoselenide positive electrode material has a wide application range and can be suitable for various metal ion battery systems such as lithium, sodium, potassium, magnesium, aluminum, calcium and the like.

Description

Chromium-based sulfoselenide positive electrode material and preparation method and application thereof
Technical Field
The invention relates to the technical field of materials, in particular to a chromium-based sulfoselenide positive electrode material and a preparation method and application thereof.
Background
With the irreversible consumption of fossil energy, new energy is becoming an indispensable part of people's lives, and the development of high-capacity novel battery electrode materials is becoming a key point in academic and industrial circles.
The transition metal chalcogenide compound has attracted extensive attention of researchers due to the characteristics of abundant synthetic raw materials, adjustable stoichiometric ratio, unique two-dimensional layered structure, convenience for ion deintercalation, occurrence of reversible chemical reaction and the like.
Disclosure of Invention
The embodiment of the invention provides a chromium-based sulfoselenide positive electrode material and a preparation method and application thereof. The chromium-based sulfoselenide positive electrode material provided by the invention has a layered structure, not only has higher specific capacity, but also has excellent rate capability, and meanwhile, the chromium-based sulfoselenide positive electrode material has a wide application range and can be suitable for various metal ion battery systems such as lithium, sodium, potassium, magnesium, aluminum, calcium and the like.
In a first aspect, an embodiment of the present invention provides a chromium-based sulfoselenide positive electrode material, including chromium-based sulfoselenide, where a chemical general formula of the chromium-based sulfoselenide is CrSxSe2-xWherein x is more than 0 and less than 2;
the chromium-based sulfoselenide positive electrode material is used as a positive electrode material of a metal ion battery, and the metal ion battery comprises any one of a sodium ion battery, a lithium ion battery, a potassium ion battery, a magnesium ion battery, an aluminum ion battery and a calcium ion battery.
Preferably, the chromium-based sulfoselenide is a two-dimensional nano-layered structure.
In a second aspect, an embodiment of the present invention provides a preparation method of the chromium-based sulfoselenide positive electrode material described in the first aspect, where the preparation method includes:
placing sodium, chromium, sulfur and selenium in a flask containing anhydrous ether under inert atmosphere, and keeping stirring; wherein the chemical general formula of the sodium, chromium, sulfur and selenium is NaCrSxSe2-x，0＜x＜2；
Dropwise adding iodine-anhydrous ether solution into the flask, observing the change of the color of the solution in the flask, stopping continuously dropwise adding when the color is not faded after the iodine-anhydrous ether solution is added, and continuously stirring for 12 hours;
and filtering the reaction product, washing the filtered reaction product with anhydrous ether, and drying in vacuum to obtain the required chromium-based sulfoselenide positive electrode material.
In a third aspect, an embodiment of the present invention provides a battery positive electrode, including the chromium-based sulfoselenide positive electrode material described in the first aspect.
In a fourth aspect, an embodiment of the present invention provides a method for preparing a battery positive electrode, where the method includes:
mixing the chromium-based sulfoselenide positive electrode material of the first aspect with a conductive agent and a binder;
adding the mixed materials into a solvent for pulping, coating the mixed materials on a conductive substrate, and drying to prepare a pole piece; or, the mixed material is directly dry-pressed into the pole piece.
Preferably, the conductive agent comprises one or more of carbon black, acetylene black, carbon nanotubes, carbon fibers, graphene or graphene oxide.
Preferably, the binder comprises one or more of polyvinyl alcohol (PVA), polyvinylidene fluoride (PVDF), Polytetrafluoroethylene (PTFE) or carboxymethylcellulose sodium (CMC).
In a fifth aspect, embodiments of the present invention provide a metal-ion battery, including the battery positive electrode of the third aspect.
The chromium-based sulfoselenide positive electrode material provided by the invention has a layered structure, fully combines the common advantages of S and Se double anions, and has high specific capacity and excellent rate capability. The material has wide application range and can be suitable for various metal ion battery systems such as lithium, sodium, potassium, magnesium, aluminum, calcium and the like.
Drawings
The technical solutions of the embodiments of the present invention are further described in detail with reference to the accompanying drawings and embodiments.
Fig. 1 is an X-ray diffraction (XRD) pattern of the chromium-based sulfoselenide cathode material prepared in example 1 of the present invention;
fig. 2 is a Scanning Electron Microscope (SEM) image of the chromium-based sulfoselenide positive electrode material prepared in example 1 of the present invention;
fig. 3 is a cycle curve diagram of the chromium-based sulfoselenide positive electrode material provided by the embodiment 2 of the invention at 0.5C in a half-cell taking lithium as a negative electrode;
fig. 4 is a graph showing the rate performance results of the chromium-based sulfoselenide positive electrode material provided in embodiment 2 of the invention in a half-cell with lithium as the negative electrode;
fig. 5 is a cycle curve diagram of the chromium-based sulfoselenide positive electrode material provided by the embodiment 3 of the invention under different multiplying powers in a half-cell taking potassium as a negative electrode.
Detailed Description
The invention is further illustrated by the following figures and specific examples, but it should be understood that these examples are for the purpose of illustration only and are not to be construed as in any way limiting the present invention, i.e., as in no way limiting its scope.
The invention provides a chromium-based sulfoselenide positive electrode material, which comprises chromium-based sulfoselenide with a two-dimensional nano-layered structure, and the chemical general formula of the chromium-based sulfoselenide positive electrode material is CrSxSe2-xWherein x is more than 0 and less than 2.
The chromium-based sulfoselenide positive electrode material can be obtained by the following preparation method, including:
step 1, sodium chromium sulfur selenium NaCrS is added in inert atmospherexSe2-x(x is more than 0 and less than 2) placing the mixture into a flask containing anhydrous ether, and keeping the stirring state;
step 2, dropwise adding iodine-anhydrous ether solution into the flask, observing the change of the color of the solution in the flask, stopping continuously dropwise adding the solution when the color is not faded any more after the iodine-anhydrous ether solution is added, and continuously stirring for 12 hours;
specifically, the reaction is finished when the color is not faded after the iodine-anhydrous ether solution is added.
And 3, filtering the reaction product, washing the filtered reaction product with anhydrous ether, and drying in vacuum to obtain the required chromium-based sulfoselenide positive electrode material.
The chromium-based sulfoselenide positive electrode material can be mixed with a conductive agent and a binder, the mixed material is added into a solvent for pulping, and the obtained product is coated on a conductive substrate and dried to prepare a pole piece; or the mixed material is directly dry-pressed into a pole piece to be used as the battery anode.
The conductive agent can comprise one or more of carbon black, acetylene black, carbon nanotubes, carbon fibers, graphene or graphene oxide; the binder may comprise one or more of polyvinyl alcohol (PVA), polyvinylidene fluoride (PVDF), Polytetrafluoroethylene (PTFE) or sodium carboxymethylcellulose (CMC).
The chromium-based sulfoselenide positive electrode material is used as a positive electrode material of a metal ion battery, and the metal ion battery can comprise any one of a sodium ion battery, a lithium ion battery, a potassium ion battery, a magnesium ion battery, an aluminum ion battery and a calcium ion battery.
In the application of the metal ion battery, the metal ion battery comprises the anode, a diaphragm, an organic electrolyte and a cathode, wherein the cathode can be one or more of metal lithium, sodium, potassium, magnesium, aluminum and calcium, or a material of which the cathode active material contains one or more ions of metal lithium, sodium, potassium, magnesium, aluminum and calcium.
The chromium-based sulfoselenide positive electrode material provided by the invention has a layered structure, fully combines the common advantages of S and Se double anions, and has high specific capacity and excellent rate capability. The material has wide application range and can be suitable for various metal ion battery systems such as lithium, sodium, potassium, magnesium, aluminum, calcium and the like.
In order to better understand the technical scheme provided by the invention, the following specific examples respectively illustrate the specific processes for preparing the chromium-based sulfoselenide positive electrode material by applying the method provided by the above embodiment of the invention, and the method for applying the same to the secondary battery and the battery characteristics.
Example 1
The embodiment provides a preparation method of a chromium-based sulfoselenide positive electrode material CrSSe.
The preparation method of CrSSe in this example includes the following steps:
(1) under the condition that a reaction system is kept in a flowing argon atmosphere, 1.86g of NaCrSSe is weighed and placed in a flask containing 20ml of anhydrous ether, and a stirring device is started to stir;
(2) dropwise adding the prepared 0.23mol/L iodine-anhydrous ether solution into the flask, observing the color change of the solution in the flask, stopping dropwise adding when the color does not fade after about 30ml of the iodine-anhydrous ether solution is added, and continuing stirring for 12 hours after the reaction is finished;
(3) and filtering the reaction product, washing the filtered reaction product with anhydrous ether, and drying in vacuum to obtain the chromium-based sulfoselenide positive material CrSSe.
The product of this example was analyzed by X-ray diffraction technique and the results are shown in FIG. 1. High and narrow diffraction peaks indicate yieldThe product has good crystallinity, and the position of diffraction peak shows that the product has the same structure as CrSe2Similar lamellar properties and no impurities are generated. As a result of scanning the product of this example with a scanning electron microscope, as shown in fig. 2, it was found that the product was formed by stacking sheet-like structures having a thickness of about 200 nm.
Example 2
The present embodiment provides a performance description of the application of the chromium-based sulfoselenide cathode material CrSSe of the above embodiment 1 in a lithium ion battery.
Mixing the product CrSSe obtained by the preparation with acetylene black and polyvinylidene fluoride (PVDF) according to the weight ratio of 8: 1:1, fully grinding, dispersing in an N-methyl pyrrolidone (NMP) solvent, uniformly mixing, smearing on an aluminum foil, drying, cutting, assembling in an argon atmosphere glove box, and assembling into a CR2032 type button cell by taking a metal lithium sheet as a counter electrode and a 1M LiTFSI solution (the solvent is 1, 3-dioxolane DOL and glycol dimethyl ether DME in a volume ratio of 1: 1) as an electrolyte. At 25 ℃, a constant current charge-discharge test is carried out at a rate of 0.5 ℃ between 1.5 and 3.5V, a cycle curve chart of the chromium-based sulfoselenide cathode material CrSSe in a half-cell taking lithium as a cathode under 0.5C is shown in fig. 3, and the first discharge capacity is 166.9mAh g-1The battery still has 89.0% capacity retention rate after 390 weeks of cycling, and thus stable cycling performance is seen. As can be seen in the rate test results shown in FIG. 4, the product can still reach 126.5mAh g even at a rate of 25C-1The capacity of the battery is released, and excellent quick-charging and quick-discharging characteristics are shown.
Example 3
This example provides a performance description of the application of the chromium-based sulfoselenide cathode material CrSSe of example 1 above in a potassium ion battery.
Mixing the product CrSSe prepared by the above steps with acetylene black and PVDF according to the weight ratio of 8: 1:1, dispersing in an NMP solvent after fully grinding, smearing on an aluminum foil after uniform size mixing, drying and cutting, assembling in a glove box in an argon atmosphere, and assembling into a CR2032 type button cell by taking a metal potassium sheet as a counter electrode and 1M KTFSI solution (the solvent is DOL and DME in a volume ratio of 1: 1) as electrolyte. The cycling results at a 0.5C rate in the voltage interval of 1.6-3.3V are shown in fig. 4, and the cycling curves of the cells are highly reversible. The first circle discharge capacity is 129.2mAh/g, namely 0.79 potassium ions are embedded, the capacity of the potassium ion battery is very high, the battery still retains 53.7mAh/g after 20 circles of circulation, and the circulation performance is relatively stable.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (9)

1. The chromium-based sulfoselenide positive electrode material is characterized by comprising chromium-based sulfoselenide, wherein the chemical general formula of the chromium-based sulfoselenide is CrSxSe2-xWherein x is more than 0 and less than 2;
the chromium-based sulfoselenide positive electrode material is used as a positive electrode material of a metal ion battery, and the metal ion battery comprises any one of a sodium ion battery, a lithium ion battery, a potassium ion battery, a magnesium ion battery, an aluminum ion battery and a calcium ion battery.
2. The chromium-based sulfoselenide positive electrode material of claim 1, wherein the chromium-based sulfoselenide is a two-dimensional nano-layered structure.
3. A method for producing a chromium-based sulfoselenide positive electrode material according to claim 1 or 2, characterized in that the method comprises:
placing sodium, chromium, sulfur and selenium in a flask containing anhydrous ether under inert atmosphere, and keeping stirring; wherein the chemical general formula of the sodium, chromium, sulfur and selenium is NaCrSxSe2-x， 0＜x＜2；
Dropwise adding iodine-anhydrous ether solution into the flask, observing the change of the color of the solution in the flask, stopping continuously dropwise adding when the color is not faded after the iodine-anhydrous ether solution is added, and continuously stirring for 12 hours;
and filtering the reaction product, washing the filtered reaction product with anhydrous ether, and drying in vacuum to obtain the required chromium-based sulfoselenide positive electrode material.
4. A positive electrode for a battery, characterized in that the positive electrode comprises the chromium-based sulfoselenide positive-electrode material according to claim 1 or 2.
5. A method for producing the positive electrode for a battery according to claim 4, comprising:
mixing the chromium-based sulfoselenide positive electrode material of claim 1 or 2 with a conductive agent and a binder;
adding the mixed materials into a solvent for pulping, coating the mixed materials on a conductive substrate, and drying to prepare a pole piece; or, the mixed material is directly dry-pressed into the pole piece.
6. The method for preparing the battery cathode according to claim 5, wherein the conductive agent comprises one or more of carbon black, carbon nanotubes, carbon fibers, graphene or graphene oxide.
7. The method of producing a battery positive electrode according to claim 6, characterized in that the carbon black comprises acetylene black.
8. The method for preparing the battery cathode according to claim 5, wherein the binder comprises one or more of polyvinyl alcohol (PVA), polyvinylidene fluoride (PVDF), Polytetrafluoroethylene (PTFE) or carboxymethylcellulose sodium (CMC).
9. A metal-ion battery comprising the battery positive electrode of claim 4.
CN202010658779.1A 2020-07-09 2020-07-09 Chromium-based sulfoselenide positive electrode material and preparation method and application thereof Active CN111916734B (en)

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CN114122389B (en) * 2021-11-26 2023-02-10 合肥工业大学 Zinc-manganese selenide solid solution positive electrode material for water-based zinc ion battery and preparation method thereof
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CN115050957B (en) * 2022-06-07 2024-01-26 深圳珈钠能源科技有限公司 Sodium ion battery positive electrode material, preparation method thereof and sodium ion battery

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CN108346783A (en) * 2018-01-11 2018-07-31 三峡大学 A kind of layered structure MoSxSe2-x/ graphene negative material and preparation method thereof
CN110233264A (en) * 2019-06-25 2019-09-13 复旦大学 A kind of sodium-ion battery positive material and preparation method thereof of stratiform sulfoselenide as high rate capability
CN110534738A (en) * 2019-08-19 2019-12-03 中南大学 A kind of dianion cobalt-based selenium sulfide and preparation method thereof
CN111206283A (en) * 2020-02-19 2020-05-29 湖南大学 Preparation and application of chromium diselenide two-dimensional material

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Publication number Priority date Publication date Assignee Title
CN108346783A (en) * 2018-01-11 2018-07-31 三峡大学 A kind of layered structure MoSxSe2-x/ graphene negative material and preparation method thereof
CN110233264A (en) * 2019-06-25 2019-09-13 复旦大学 A kind of sodium-ion battery positive material and preparation method thereof of stratiform sulfoselenide as high rate capability
CN110534738A (en) * 2019-08-19 2019-12-03 中南大学 A kind of dianion cobalt-based selenium sulfide and preparation method thereof
CN111206283A (en) * 2020-02-19 2020-05-29 湖南大学 Preparation and application of chromium diselenide two-dimensional material

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